反应详情

A solution of tert-butyl 3-((8-(4-(4-methoxyphenyl)-4-oxobutyl)-4-oxo-1-phenyl-1,3,8-triazaspiro[4.5]decan-3-yl)methyl)benzoate (100 mg, 0.496 mmol, 1 equiv) in 4M hydrogen chloride solution in dioxane was stirred at ambient temperature for 4 h. The mixture was concentrated in vacuo and the crude residue was purified using preparatory high performance liquid chromatography to afford the acetate salt of the title compound as a white solid (67 mg, 74%); 1H NMR (400 MHz, DMSO-d6): δ 1.78 (bs, 2H); 1.95 (bs, 2H); 2.52-2.54 (m, 3H); 2.76 (bs, 4H); 3.08 (bs, 3H); 3.84 (s, 3H); 4.62 (s, 2H); 4.63 (s, 2H); 6.78 (d, 1H, J=7.2 Hz); 6.93 (bs, 2H); 7.05 (d, 2H, J=9.2 Hz); 7.20 (t, 2H, J=7.6 and 7.2 Hz); 7.49-7.57 (m, 2H); 7.87-7.89 (m, 2H); 7.96-7.98 (m, 2H); 12.45 (s, 1H); MS for C32H35N3O5 m/z 542.02 (M+H)+.

1. concentrationThe mixture was concentrated in vacuo
2. customthe crude residue was purified